Industrial production method for preparing nanometer lithium iron phosphate by adopting solvent thermal method

A technology of lithium iron phosphate and solvothermal method, which is applied in nanotechnology, chemical instruments and methods, phosphorus compounds, etc., can solve problems such as uneven and wide particle size distribution, poor product batch consistency, and poor electrochemical performance of products , to achieve the effects of good recovery and purification efficiency, easy control, and excellent electrochemical performance

Inactive Publication Date: 2013-04-10
BEIJING EASPRING MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the mainstream lithium iron phosphate production method is the high-temperature solid-phase method. Although this method is simple to operate and easy to produce, the sintered product has large primary particles, serious agglomeration, and uneven and wide particle size distribution, which leads to the diffusion of lithium ions. The channel is too long, the electrochemical performance of the product is poor, and the product batch consistency is poor, etc.

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  • Industrial production method for preparing nanometer lithium iron phosphate by adopting solvent thermal method
  • Industrial production method for preparing nanometer lithium iron phosphate by adopting solvent thermal method

Examples

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Embodiment 1

[0027] Phosphoric acid, ferrous sulfate, lithium hydroxide, glucose, H 2 O and isopropyl alcohol are mixed and stirred evenly in a closed reaction kettle, the molar ratio of phosphoric acid, ferrous sulfate, and lithium hydroxide is 1:1:3, and the mass of the solid accounts for 30% of the total mass of the solution. Water and isopropyl The volume ratio of alcohol is 1: 5, wherein the glucose addition is 13% of the mass of solid powder (excluding carbon source); the airtight reactor is protected by an inert atmosphere, and after stirring for 2 hours, the temperature is raised to 200° C., and the heating time is 3 hours. Make it undergo a crystallization reaction, and the water vapor is condensed and recovered through the condensation system installed on the reactor; after cooling, it is centrifugally settled, and then washed with isopropanol, and this cycle is repeated several times until the impurities on the particle surface are removed; the impurity-removed The slurry is spr...

Embodiment 2

[0033] Mix ammonium phosphate, ferrous chloride, lithium oxalate, salicylic acid, and absolute ethanol in a closed reaction kettle and stir evenly. The molar ratio of ammonium phosphate, ferrous chloride, and lithium oxalate is 1:1:4. Wherein the salicylic acid addition is 18% of solid powder (does not contain carbon source) quality, and the quality of solid accounts for 80% of total solution mass; Airtight reactor inert atmosphere protection, after stirring time 5h, be warming up to 100 ℃, heating The time is 6 hours, so that crystallization reaction occurs; after cooling, it is separated by pressure filtration, and then washed with absolute ethanol, and this cycle is repeated several times until the impurities on the surface of the particles are removed; the slurry from which impurities are removed is spray-dried to obtain two The secondary particles are spherical powders; the waste water and waste organic solvents generated during the synthesis process are recovered and puri...

Embodiment 3

[0038] Ammonium dihydrogen phosphate, ferrous oxalate, lithium carbonate, carbon nanofiber, H 2 O and propanol are mixed and stirred evenly in a closed reaction kettle, the molar ratio of ammonium dihydrogen phosphate, ferrous oxalate, and lithium carbonate is 1:1:2, and the mass of the solid accounts for 55% of the total mass of the solution. The volume ratio of alcohol is 1:1.5, wherein the amount of carbon nanofiber added is 7% of the mass of the solid powder (without carbon source); the closed reaction kettle is protected by an inert atmosphere, and after stirring for 7 hours, the temperature is raised to 300° C., and the heating time is 1 hour , so that crystallization reaction occurs, and the water vapor is condensed and recovered through the condensation system installed on the reactor; after cooling, it is separated by pressure filtration, and then washed with propanol, and this cycle is repeated several times until the impurities on the surface of the particles are rem...

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Abstract

The invention discloses an industrial production method for preparing nanometer lithium iron phosphate by adopting a solvent thermal method. The industrial production method comprises the following steps that phosphorus source compounds, iron source compounds, lithium source compounds, carbon sources and solvents are proportionally and sequentially added into a sealed reaction kettle and are uniformly mixed and stirred, the stirring temperature rising reaction is carried out in inert atmosphere, primary products of the lithium iron phosphate are obtained, solid and liquid separation is carried out, washing and drying are carried out, the roasting is carried out in the inert atmosphere, and the lithium iron phosphate products are obtained. Waste water and waste organic solvents generated in the production process are recovered and reutilized through reduced pressure distillation. The obtained product of the lithium iron phosphate materials has fine primary particle size and narrow particle size distribution, in addition, the distribution is uniform, the conductivity is good, the electrochemical performance of products is good, the product batch consistency is good, the operation of a recovery method is simple, the control is easy, the energy consumption is low, and the method is suitable for industrial production and application.

Description

technical field [0001] The invention relates to a production method of lithium ferrous phosphate material for lithium ion power batteries, in particular to an industrial production method of nanoscale lithium iron phosphate for lithium ion power batteries prepared by a solvothermal method. Background technique [0002] As an emerging power source, lithium-ion batteries have many advantages such as high voltage, high capacity, light weight, small size, safety and environmental protection, and are widely used in mobile phones, notebook computers, digital products and other fields. With the increasing energy crisis, The application of lithium-ion batteries in new energy vehicles has gradually become a hot research field. At present, most commercial batteries use lithium cobaltate as the cathode material. However, due to the lack of cobalt resources, lithium cobaltate has problems such as high material price and safety. Therefore, people have been developing other lithium-ion ba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58B82Y40/00
CPCY02E60/12Y02E60/10
Inventor 秦波龚金保陈彦彬李鸿儒
Owner BEIJING EASPRING MATERIAL TECH CO LTD
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